Synthesis · Field-Effect Transistor Based on an in Situ Grown Metal-Organic Framework Film as a Liquid-Gated Sensing Device

9 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: SI

Route 1: Drop Cast

p002 / SI p.S-2 · Drop-casting method · Figure S5d-f

Metal precursorsNi-MOF product prepared from NiCl2*6H2O under similar chemistry

Linker precursorsNi-MOF product prepared from HATP*6HCl under similar chemistry

SolventsDI water and ethanol for centrifugation/washing; ethanol for dispersion

AtmosphereOpen heated for reaction; vacuum oven drying and baking

Temperature65 reaction; 100 drying/baking

Time2 h reaction; 12 h powder drying; 2 h device baking

Substrate orientationDrop-cast onto FET channel

Work-upReacted product centrifuged three times with DI water and ethanol, dried in vacuum oven at 100 C for 12 h, mixed with ethanol, dropped onto FET channel, and baked at 100 C for 2 h.

Scalability contextDrop-cast nanosheets stacked into a non-uniform mass and adversely affected FET properties.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	dried Ni-MOF powders	appropriate amount	p002 / SI p.S-2 · Drop-casting method · Figure S5d-f
Solvent	ethanol	dispersion and washing solvent	p002 / SI p.S-2 · Drop-casting method · Figure S5d-f
Solvent	DI water	washing solvent	p002 / SI p.S-2 · Drop-casting method · Figure S5d-f

Complete recipeSource: Main

Route 2: Other

p002 / article p.35936 · Experimental Section - Fabrication of the FET Device

Metal precursorsAu source/drain electrodes, 100 nm; Ti adhesion layer, 10 nm

SolventsAcetone; DI water; ethanol

AdditivesPhotoresist used for lithography/lift-off; silicon rubber well added after MOF growth for liquid testing

AtmosphereAmbient processing; final drying at 100 C

Temperature100

Time2

Substrate orientationSi (500 nm)/SiO2 (300 nm) wafer, 2.5 x 2 cm; channel length 50 um and width 1000 um

Work-upUltraviolet lithography and lift-off, magnetron sputtering of Ti/Au, brief ultrasonic acetone treatment, rinsing with DI water and ethanol, drying at 100 C for 2 h.

ActivationUV ozone treatment for about 1 h before MOF growth

Scalability contextDevice dimensions are explicitly reported; no scale-up beyond 2.5 x 2 cm wafer was demonstrated.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Si (500 nm)/SiO2 (300 nm) wafer	2.5 x 2 cm	p002 / article p.35936 · Experimental Section - Fabrication of the FET Device
Other	Ti layer	10 nm	p002 / article p.35936 · Experimental Section - Fabrication of the FET Device
Other	Au layer	100 nm	p002 / article p.35936 · Experimental Section - Fabrication of the FET Device
Solvent	acetone	ultrasound for a few seconds	p002 / article p.35936 · Experimental Section - Fabrication of the FET Device
Solvent	DI water and ethanol	rinse	p002 / article p.35936 · Experimental Section - Fabrication of the FET Device

Partial recipeSource: Both

Route 3: Other

p004 / article p.35938 · Result and Discussion · Table 1 and Figure S8

Metal precursorsNiCl2*6H2O (6.6 mg, 0.019 mmol)

Linker precursorsHATP*6HCl (10.0 mg, 0.028 mmol)

SolventsDI water; DI water and ethanol for washing

AdditivesNH3*H2O, 0.3 mL

AtmosphereOpen heated in water bath; atmosphere otherwise not specified

Temperature65

Time2

Substrate orientationCleaned FET suspended upside-down at the liquid surface of the reaction solution

Work-upSame in situ procedure as shorter-time devices; detailed washing/drying inferred from main experimental route.

ActivationUV ozone pretreatment before MOF growth.

Scalability contextLonger reaction damaged Au electrodes and decreased electrical performance.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*NiCl26H2O**	6.6 mg, 0.019 mmol	p004 / article p.35938 · Result and Discussion · Table 1 and Figure S8
Linker	*HATP6HCl**	10.0 mg, 0.028 mmol	p004 / article p.35938 · Result and Discussion · Table 1 and Figure S8
Base	*NH3H2O**	0.3 mL	p004 / article p.35938 · Result and Discussion · Table 1 and Figure S8

Complete recipeSource: Both

Route 4: Other

p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device

Metal precursorsNiCl2*6H2O (6.6 mg, 0.019 mmol)

Linker precursorsHATP*6HCl (10.0 mg, 0.028 mmol)

SolventsDI water, 5 mL for nickel solution and 5 mL for linker solution; DI water and ethanol for washing

AdditivesNH3*H2O, 0.3 mL

AtmosphereOpen heated in water bath; atmosphere otherwise not specified

Temperature65

Time0.25

Substrate orientationCleaned FET suspended upside-down at the liquid surface of the reaction solution

Work-upCool to room temperature; wash with a large amount of DI water and ethanol multiple times; dry in vacuum oven at 100 C for 2 h.

ActivationFET pretreated by UV ozone cleaner for about 1 h to remove organic impurities and increase hydroxyl groups.

Scalability contextNo scale-up study reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*NiCl26H2O**	6.6 mg, 0.019 mmol	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Linker	*HATP6HCl**	10.0 mg, 0.028 mmol	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Base	*NH3H2O**	0.3 mL	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Solvent	DI water	10 mL total	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device

Complete recipeSource: Both

Route 5: Other

p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device

Metal precursorsNiCl2*6H2O (6.6 mg, 0.019 mmol)

Linker precursorsHATP*6HCl (10.0 mg, 0.028 mmol)

SolventsDI water, 5 mL for nickel solution and 5 mL for linker solution; DI water and ethanol for washing

AdditivesNH3*H2O, 0.3 mL

AtmosphereOpen heated in water bath; atmosphere otherwise not specified

Temperature65

Time0.5

Substrate orientationCleaned FET suspended upside-down at the liquid surface of the reaction solution

Work-upCool to room temperature; wash with a large amount of DI water and ethanol multiple times; dry in vacuum oven at 100 C for 2 h.

ActivationFET pretreated by UV ozone cleaner for about 1 h to remove organic impurities and increase hydroxyl groups.

Scalability contextNo scale-up study reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*NiCl26H2O**	6.6 mg, 0.019 mmol	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Linker	*HATP6HCl**	10.0 mg, 0.028 mmol	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Base	*NH3H2O**	0.3 mL	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Solvent	DI water	10 mL total	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device

Complete recipeSource: Both

Route 6: Other

p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device

Metal precursorsNiCl2*6H2O (6.6 mg, 0.019 mmol)

Linker precursorsHATP*6HCl (10.0 mg, 0.028 mmol)

SolventsDI water, 5 mL for nickel solution and 5 mL for linker solution; DI water and ethanol for washing

AdditivesNH3*H2O, 0.3 mL

AtmosphereOpen heated in water bath; atmosphere otherwise not specified

Temperature65

Time0.083

Substrate orientationCleaned FET suspended upside-down at the liquid surface of the reaction solution

Work-upCool to room temperature; wash with a large amount of DI water and ethanol multiple times; dry in vacuum oven at 100 C for 2 h.

ActivationFET pretreated by UV ozone cleaner for about 1 h to remove organic impurities and increase hydroxyl groups.

Scalability contextAuthors report large-area, uniform film formation on the wafer, but no independent scale-up study.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*NiCl26H2O**	6.6 mg, 0.019 mmol	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Linker	*HATP6HCl**	10.0 mg, 0.028 mmol	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Base	*NH3H2O**	0.3 mL	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Solvent	DI water	10 mL total	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Solvent	ethanol	wash solvent	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device

Complete recipeSource: Both

Route 7: Other

p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device

Metal precursorsNiCl2*6H2O (6.6 mg, 0.019 mmol)

Linker precursorsHATP*6HCl (10.0 mg, 0.028 mmol)

SolventsDI water, 5 mL for nickel solution and 5 mL for linker solution; DI water and ethanol for washing

AdditivesNH3*H2O, 0.3 mL

AtmosphereOpen heated in water bath; atmosphere otherwise not specified

Temperature65

Time1

Substrate orientationCleaned FET suspended upside-down at the liquid surface of the reaction solution

Work-upCool to room temperature; wash with a large amount of DI water and ethanol multiple times; dry in vacuum oven at 100 C for 2 h.

ActivationFET pretreated by UV ozone cleaner for about 1 h to remove organic impurities and increase hydroxyl groups; silicon rubber well added after drying for liquid tests.

Scalability contextThe film almost completely covered the silicon wafer surface; no larger scale was tested.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*NiCl26H2O**	6.6 mg, 0.019 mmol	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Linker	*HATP6HCl**	10.0 mg, 0.028 mmol	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Base	*NH3H2O**	0.3 mL	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Solvent	DI water	10 mL total	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Solvent	ethanol	wash solvent	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device

Partial recipeSource: Main

Route 8: Other

p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device

Metal precursorsNiCl2*6H2O (6.6 mg, 0.019 mmol)

Linker precursorsHATP*6HCl (10.0 mg, 0.028 mmol)

SolventsDI water; DI water and ethanol for washing

AdditivesNH3*H2O, 0.3 mL

AtmosphereOpen heated in water bath; atmosphere otherwise not specified

Temperature65

Time1

Substrate orientationPure Si/SiO2 wafer without gold plating

Work-upSame procedure as Au-patterned in situ samples; washing and drying as described for Ni-MOF-FET.

ActivationUV ozone treatment presumed from same procedure.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*NiCl26H2O**	6.6 mg, 0.019 mmol	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Linker	*HATP6HCl**	10.0 mg, 0.028 mmol	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device
Base	*NH3H2O**	0.3 mL	p003 / article p.35937 · Experimental Section - Fabrication of the Ni-MOF-FET Device

Complete recipeSource: SI

Route 9: Other

p002 / SI p.S-2 · Scooping-up method · Figure S5a-c

Metal precursorsNiCl2*6H2O (6.6 mg, 0.019 mmol)

Linker precursorsHATP*6HCl (10.0 mg, 0.028 mmol)

SolventsDI water, 5 mL for nickel solution and 5 mL for linker solution

AdditivesNH3*H2O, 0.3 mL

AtmosphereOpen heated in water bath; atmosphere otherwise not specified

Temperature65

Time0.25

Substrate orientationCleaned Au-patterned Si/SiO2 wafer used to transfer film after cooling

Work-upAfter cooling to room temperature, film was transferred to wafer and dried in a vacuum oven at 100 C for 2 h.

Scalability contextTransfer route gave cracked films and poor electrical properties.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*NiCl26H2O**	6.6 mg, 0.019 mmol	p002 / SI p.S-2 · Scooping-up method · Figure S5a-c
Linker	*HATP6HCl**	10.0 mg, 0.028 mmol	p002 / SI p.S-2 · Scooping-up method · Figure S5a-c
Base	*NH3H2O**	0.3 mL	p002 / SI p.S-2 · Scooping-up method · Figure S5a-c
Solvent	DI water	10 mL total	p002 / SI p.S-2 · Scooping-up method · Figure S5a-c